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A method for filling activated carbon in carbon fiber prefabricated body and its application

A carbon fiber preform and activated carbon technology, which is applied in the field of high-reactivity C/C preform preparation, can solve the problems of low cracking yield of precursors, inconvenient enlargement of high-pressure vessels, increased processes, etc., to meet the requirements of low cost, short cycle, The effect of solving equipment amplification bottlenecks and solving security problems

Active Publication Date: 2021-05-18
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the CVI process, due to the concentration gradient of the silicon-containing gas, the deposition rate outside the preform is greater than that inside the preform, so crusting occurs, and the surface of the preform needs to be processed multiple times to open the pores before proceeding. Deposition, resulting in an increase in the process, prolonging the preparation cycle, and increasing the production cost
The disadvantages of the PIP process are the high cost of raw materials, and the low cracking yield of the precursor, which requires repeated immersion-cracking to achieve densification
However, the biggest problem faced by the existing LSI process is that the amount of SiC generated after reaction sintering is small, and a large amount of silicon and carbon remain in the composite material. reduced performance
At the same time, due to the large amount of silicon remaining in the composite material, its use temperature is also limited.
[0004] In order to solve the problem of poor mechanical properties of C / SiC composite materials in the LSI process, the Institute of Metal Research, Chinese Academy of Sciences invented "a reactive infiltration process for C / SiC composite materials (application number 201318009258.4)", which uses solvothermal technology. The method of preparing activated matrix carbon in the carbon fiber prefabricated body makes the matrix carbon react completely with liquid silicon, eliminates residual carbon, reduces residual silicon content, reduces the reaction temperature at the same time, reduces the thermal damage and chemical damage of carbon fiber itself, thereby greatly improving LSI Mechanical Properties of C / SiC Composites Prepared by Process
However, in the activated carbon filling process of this process, the polymerization temperature of the resin is 100-240°C. At this time, the internal pressure of the reactor is 0.3-6MPa. The high operating pressure not only brings production safety risks, but also the enlargement of the high-pressure vessel is extremely inconvenient. Bottlenecks restricting the scale-up of the process

Method used

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  • A method for filling activated carbon in carbon fiber prefabricated body and its application
  • A method for filling activated carbon in carbon fiber prefabricated body and its application
  • A method for filling activated carbon in carbon fiber prefabricated body and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Pretreatment of Aminophenolic Resin

[0039] 1) Pre-evaporation of phenolic resin

[0040] First, take 100ml of phenol-formaldehyde resin, put it in a flask, and evaporate it with a rotary evaporator at 60° C. and 1000 Pa for 40 minutes to remove 50-70 wt % of the solvent in the liquid phenol-formaldehyde resin.

[0041] 2) Preparation and drying of phenolic resin solution

[0042] Add 40ml of acetone to the pre-evaporated phenolic resin, stir evenly, and dry it with a spray dryer. The temperature of the hot argon gas is 80°C, and the feeding speed is 5ml / min. The dried phenolic resin becomes powder.

Embodiment 2

[0044] Atmospheric pressure crosslinking and curing of phenolic resin in different solvent systems to prepare activated carbon

[0045] 1) Prepare phenolic resin solution

[0046] First prepare the phenolic resin organic solution, get 40g of the phenolic resin powder prepared in Example 1 and dissolve them in 100ml glycerol (chemically pure), 90ml glycerin+10ml dimethyl sulfoxide mixed solution or 85ml glycerin+10ml dimethyl sulfoxide+ 5g polyether mixed solution, a transparent liquid was obtained after thorough stirring.

[0047] 2) Preparation of polymer by in situ polymerization

[0048] Pour the above solution into a 150ml glass bottle, put it into an electric heating constant temperature drying box to heat, the reaction temperature is 160°C, the holding time is 12 hours, and cool to room temperature.

[0049] 3) Washing, drying and grinding

[0050] The reaction product obtained in step 2) is soaked in ethanol or deionized water for 1-2 hours, filtered, dried in a cons...

Embodiment 3

[0054] Atmospheric pressure assembly of activated carbon in carbon fiber prefabricated body

[0055] 1) Prepare phenolic resin solution

[0056] First prepare the phenolic resin organic solution, take 40g of the phenolic resin powder prepared in Example 1 and dissolve in 85ml of glycerin+10ml of dimethyl sulfoxide+5g of polyether mixed solution, after fully stirring, a transparent liquid is obtained.

[0057] 2) Atmospheric pressure filled activated carbon

[0058] The needle-punched carbon fiber preform was immersed in the phenolic resin solution prepared in step 1) by vacuum impregnation, and then placed in a polytetrafluoroethylene beaker, kept at 160°C for 12 hours, and then cooled to room temperature; the carbon fiber preform was taken out in the Perform pyrolysis at 900°C for 2 hours to obtain an activated carbon matrix; repeat the above vacuum impregnation-solvothermal polymerization-pyrolysis process 6 times to obtain a carbon fiber preform filled with an activated ca...

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Abstract

The invention belongs to the technical field of preparation of high-reactivity C / C prefabricated bodies, in particular to a method for filling activated carbon in carbon fiber prefabricated bodies and its application. Dry the liquid aminophenol-formaldehyde resin to remove part of the solvent, then dissolve it in an organic solvent in a certain proportion, make a resin solution with a small amount of additives or no additives, impregnate the carbon fiber preform in the resin solution, and place it in an oven In-situ cross-linking polymerization at normal pressure; the polymerized product is taken out, washed with ethanol, dried, and pyrolyzed under vacuum or inert atmosphere to obtain a porous C / C composite material. The density of the composite material can be adjusted by repeated dipping times. The C / C composite material prepared by the method of the invention has good reaction performance with silicon and silicon alloys, and the C / SiC composite material with high performance and low cost can be prepared through reaction infiltration.

Description

technical field [0001] The invention belongs to the technical field of preparation of high-reactivity C / C prefabricated bodies, in particular to a method for filling activated carbon in carbon fiber prefabricated bodies and its application. Background technique [0002] C / SiC ceramic matrix composites have the advantages of high specific strength, high specific modulus, low density, high thermal conductivity, low thermal expansion and good thermal shock resistance, and can be widely used as thermal protection, thermal structure and friction braking materials Aerospace, energy, transportation and other fields. In addition, C / C composite materials have the characteristics of high specific strength, low density, low thermal expansion coefficient, and excellent high-temperature mechanical properties, and are regarded as one of the key materials in the aerospace and national defense fields. However, this material is prone to oxidation and ablation in the environment of high-temp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/83C04B38/00C04B35/622
CPCC04B35/622C04B35/83C04B38/0032C04B2235/48C04B2235/96C04B38/0054C04B38/0067
Inventor 张劲松徐兴祥石小磊
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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